DE1958691A1 - Process for making sugar - Google Patents

Description

W.R. Grace 4 Co. (Prio November 26, 1968 -

IF. 56144/68 - 14141 - 6649) New York, N.Y./V.St.A.

Hamburg, November 20, 1969 Process for making sugar

The present invention relates to a method for producing cane sugar or beet sugar or Sucrose and the products thus obtained. These products may or may not contain noticeable proportions Contain invert sugar, depending on the one used Source material.

In the usual processes for the production of sucrose is obtained from cane sugar or from sugar beet Raw juice first decolorized and then desalinated. The cleared one Syrup is then evaporated and a fractional crystallization in several precisely adhered to process steps subjected, being a caramelization by working is suppressed under vacuum to reduce the evaporation temperature. A fractional crystallization is essential, since an inversion of the cane sugar takes place during processing, which is usually up to 15 ow.Ji the original sucrose content to the final

Processing matters · This essentially non-crystallizable invert sugar is discarded together with up to 20% non-recoverable sucrose and is processed as animal feed or for lower-quality sugar products such as molasses.

It has now been found that the raw syrup or a syrup with. noticeable proportions of invert sugar up to solid State can be evaporated and an essentially complete isolation of the sugar content in one for Form suitable for human use · These products are hereinafter referred to as edible sugars im In contrast to those only suitable for pre-feeding inferior quality products.

According to the invention, a sucrose solution and fine sucrose particles are dispersed in separate streams in a hot air stream so that the particles are coated with the solution and the water evaporates in the latter and a solid product is obtained. The isolation of the sucrose is essentially 100 % and, beyond that, there is practically no inversion of the sucrose in the refining process. The process can be applied to raw cane sugar syrup or to a syrup which contains significant amounts of invert sugar,

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such as a mother liquor from one of the fractional crystallization stages of the usual sugar production. In the first case, the final product consists of microcrystalline sucrose »while in the latter that Product consists of microcrystalline sucrose »which is embedded in an amorphous matrix consisting of a mixture of sucrose and invert sugar. This matrix corresponds very well to the non-crystallizable one Product obtained at the end of numerous fractional crystallizations in the usual zuoker manufacturing process

Figures 1, 2 and 3 of the accompanying drawings are Photomicrographs, namely show »

Flg. 1 - a commercial cane sugar * of the 100

is crystalline and wherein each individual particle is a single crystal, and

Flg. 2 and 3 - corresponding photomicrographs as

founding geroässen product in which a Syrup with a content of sucrose and invert sugar is used as a starting product became. These products are agglomerates in the order of about 1,000 / u what the size of the individual crystals of the

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Commercially available cane sugar corresponds to down to about 50 ai. The agglomerates consist of agglomerated microcrystals of sucrose, which are held together by a matrix which consists essentially of an amorphous matrix of invert sugar and sucrose.

If clarified boiled syrup is used as the starting material, the product consists almost entirely of agglomerates from microcrystalline sucrose.

The erfindungsgeraässen products are free flowing Peststoffe, isid stored which as crystallized sucrose merchantable quality "can ground * Hers freiflieSenäe condition w \ u slight solubility" used sslrt them particularly suitable for the production of chocolate and other confectionery, and for the production of beverages. The agglomerates can SiOH easily crush end break very quickly with a simple mixing process to «They can therefore directly as agglomerates there eing" s "did expectant" i, where it was previously required £ # iQTerteilter 2ack "r" Bine investigation aw old nasii of products & Diffrafctioisverfalir «! It is evident that the one crystal structure of 43 Ma possesses about 85 ^ · Man kaan

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excellent edible products from a raw material get what up to 20 # invert sugar, based on contains the total sugar content. The bulk density of the Products manufactured according to the invention differs significantly from commercially available crystallized sucrose. The latter has a rubble density of about 22.8 to 25 kg per 28.3 liters, while the bulk density of the products produced by the process according to the invention 12.5 to 19.5 kg per 28.5 liters.

It is an essential feature of the process according to the invention that the solid sugar used is present in sufficient quantity during drying and is sufficiently fine so that there is sufficient surface to absorb all of the syrup droplets as a thin layer on the surface of the solid constituents the solid sugar should be distributed as evenly as possible within the spray device. In this way, the evaporation of the water from the syrup can take place very quickly. The sticking together of several solid particles by the syrup and a consequent shielding of the syrup against evaporation by means of hot air is reduced to a minimum. In practice it has been found that when using an aqueous mixture or a syrup with a content of 60 to 70 Qev. a ver

ORIGINAL BATHROOM

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ratio of 1ί3 and preferably 2: 3 parts by weight Finely divided solid sugar to 1 part by weight of solid syrup gives good results. Other concentrations of syrup can be used »such as solutions« which contain up to 80 to 90 weight percent sugar. Such Solutions must be used hot to prevent premature crystallization. Preheating the syrup ) is generally advisable as it is more economical to preheating the syrup as supplying the same amount of heat in the form of hot air. Preheating the syrup also lowers its viscosity so that finer droplets are formed.

If the method according to the invention is started, so can or should the solid particles by recycling part of the end product, optionally after light . Grinding are fed, so that agglomerates are broadened with an undesirable size. At the beginning of the process *, commercially available sucrose is used or give trap a supply of the manufactured according to the invention Product from a previous operation. When using commercial sugar as the starting product, the Concentration of commercial sugar gradually reduced «by switching the system to circulation mode *

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The flow rate and the temperature of the hot air are determined in that the solidification or crystallization of the syrup prefers possible far until the syrup entraining particles have their way into the SprUhtrocknungskatmner terminated "Practically, temperatures on the order of 100 to 150 ⁰ C for uses the inlet air with good results. For practical reasons, it is better to adjust the temperature of the incoming air and its speed of passage through the chamber, the exiting air has a temperature in a range of 55 to 75 ⁰ C possesses · Here, a discoloration of the final product almost completely prevented. In the first stages of the process, overheating is prevented by cooling due to the evaporation of water

A is preferably used for the method according to the invention Centrifugal spray dryer as shown in Fig. 4 was used This spray dryer 1 has a centrifugal spray disk 2, which is attached to a shaft 2 on the cover kept and on suitable catfish, for example as at a drive pulley 6 is driven via the line 7 air is fed into the tower from a heater 8, and either by suction from the supply side of the tower or by a fan in the heating cable. Aue a fore

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Storage tank 9 becomes syrup at a measured speed with a feed pump 10 in a tub in the top the disk 2 promoted. Two or more bores lead radially from this trough to the outer edge of the disc The bores end in small metal tubes 11 with an inner diameter of about 2 to 4 mm. A screw conveyor 12 guides the circulated sugar at a predetermined rate to a point just above the level of the rotating disk 2 and the air currents generated by the rotation distribute the powder more or less evenly in the spray of the syrup droplets that are thrown off the disc. In the upper area of the Device can be provided with a distributor or baffle plate so that the powder falls down in a circular manner and a cylindrical rain of particles outside the circulation route of the tubes 11 of the disc 2 forms.

The tower 1 tapers conically at its lower end and Is connected to a Saramel vessel 14 via a discharge line 13 A secondary line 15 leads to a separating cyclone 16, which retains the finest particles in the product and also serves to draw air through the system.

During operation, good results are achieved with the rotational speed, of the pulley corresponding to a circumferential speed

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ness obtained at the outer ends of the tubes 11 8000-11000 m / mln with a syrup containing about 70 sugar. Greater speeds of rotation are advisable in the case of more viscous syrups which contain, for example, 80 to 90% by weight of sugar.

Other spray disks with a circumferential flange and a series of right-angled holes with dimensions of 6 χ 12 mm for a Schelbendurohmesser 150 mm and about 50 holes can also be used will·

The powdered sugar that went into the pan inside the circumferential flange has been promoted, is thrown through dl · radial bores outwards, which leads to leads to an extremely uniform particle distribution. The syrup is fed into a Within the main part of the disc and conveyed by centrifugal force through the bores of the chamber Peripherals sprayed on. The peripheral speed is at this arrangement is about the same as that of the above device when using the device shown in FIG the removal of water from the syrup takes place almost completely within an extremely short period of time. A dwell time a few seconds in the device is sufficient.

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On the other hand, the crystallization is somewhat delayed · As a result, part of the mass thrown against the vessel wall adheres to it · However, as the crystallization progresses, the product adhering to the wall flakes from and falls down. This material consists of comparatively large agglomerates ^ which have ended Crystallization can be broken up easily «The remaining material flows evenly into the tower from below and sees a sight glass when looking at it like a small blizzard · The material settling on the ground can easily be in the form of small agglomerates with a particle size of generally less than 1 mm and in the form of finely divided powder to be sucked off · If the crystallization during discharge of the product is not yet complete, the product crystallizes and solidifies quickly in air or when blowing cooling air over the in thinner Layer of spread product.

Although the centrifugal spray guns are preferred, nozzle devices can also be used »To be used for spraying.

As already mentioned, the product falls in the form of a finely divided powder or in lumps which are easy to disintegrate.

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smaller · This product has significant advantages in chocolate production, both in terms of the quality of the end product and in terms of its quality easier processing, especially when refining " The new product can be processed relatively easily with liquid cocoa or liquid chocolate, what on the small particle size, the better flowability, the higher dispersion rate, the Porosity, the low bulk density of the agglomerates and is based on the fact that the new products show no tendency to stick together.

The novel solubility properties of the present Sugar products are easily identified by tasting a small amount with your tongue. The solution happens so quickly that you get the impression of a slight Sharpness has * although the sweetening power is the same as sucrose 1st · These same properties facilitate also processing the sugar with other foods

The process according to the invention can be used for production of particulate »sugars from numerous raw materials, such as edible molasses, raw sugar syrup, beet or sugar cane syrup. Furthermore, one can

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in the process according to the invention, use sugar solutions which are obtained in conventional sugar refining after the second, third or last crystallization stage. In cases where a pure white product is desired, the starting product should be decolorized with activated charcoal and desalting, for example. The starting products can also be adjusted by evaporation or dilution to a concentration that is suitable for the process with the existing system. It was noted "that in general the starting syrup about 1 to 20 <f> invert sugar, based on the total sugar content in the syrup contains.

In contrast to conventional processing methods in sugar production, the present method does not involve any substantial inversion of the sucrose originally present in the syrup. If a starting product with a given concentration of invert sugar is used, the invert sugar content does not increase in the process according to the invention. With the new process, practically all of the sugar in the given starting product can be obtained. This is in contrast to the usual sucrose production processes, in which several crystallization steps are required for concentration and only about 70 to 80 % of the sucrose originally present is obtained in edible quality

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will. Up to now, $ 20 to $ 30 of the sugar contained in cane sugar juice had to be otherwise recycled as waste products unsuitable for human consumption. -

example 1

Bs were different test series with different Sugar syrups carried out. Here-became a Spray device according to FIG. 4 used · Overall eleven test series were carried out, the work of which » conditions in the following table I are given. In experiment 1, the added liquid contained Component water without further addition of sucrose or invert sugar. In experiment 2, a syrup was used which contained only sucrose. In the trials 5 to 7 a syrup was used which contained sucrose together with various amounts of invert sugar In bequests 1 through 5, sucrose was used as an initial one added solid used in the spray dryer.

Trials 8, 9, 10 and 11 were different natural sugar solutions such as dissolved raw sugar, refined cane sugar syrup and raw cane sugar syrup are used. In experiments 7 »8, 9, 10 and 11 that came first used circulated · Material from previous experiments

0 0 9 8 2 5/1353 ^{BAD 0RSGINAL}

195

used when starting the experiment. In all experiments the circulation ratio was about 3 parts by weight of solid material and 1 part by weight of pesticides in the syrup solution. In order to check the progress of the spray drying during test b, several returns, as indicated in the last column of Table 1, were carried out. In the case of a return, the system was charged with 45.5 kg of dry material at a return ratio of 2: 1. Then, on the next return, an amount of 45.5 kg of the dry material from the previous process was sent through the plant.

In the following table, in experiment No. 8 raw sugar "in experiment Kr" 9 refined cane sugar, in experiment Kr. 10 a high-grade syrup and in experiment Hr, II a Hohrsueker raw syrup was used. The material of the first return passed in experiments 1 to 6 from sucrose, in case of failure 7 * 8 ^ £ & 9 "as &&& product of the ¥ er ^ aiuehes Nr. 4" in experiment 10 from the product of the versuohee 4 usd 6 and in experiment 11 from around product experiments 6, 9 and 10 *

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Table I. Bloom product ; Temperatures in C

Test syrup invert air volume on-off insert tower product test number of No. ⁰ Bx sugar in ηκ / hour. step material in return

in % air air hours

° 5
tar

10

11th

68

70

69

68

67

69

70

68

68

70

0 0

7.25 14.6 19.2

5.6

15.1 4.0

23.1 0.58

3.5

2 200 2 200 2 200 2 200 2 200 1 500

1 600

2 100 2 100 2 100 2 100

135 60 20th 130 72 Ι4θ 70 55 112 80 110 45 75 80 65 110 45 70 80 65 110 45 80 85 85 185 105 70 - 85 150 90 70 95 70 120 60 80 100 80 110 55 80 90 80 110 55 75 85 75 115 60 80 90 75

0.6

5.3 5 5 4.6

4.3 19th 4.2 2 2 2.5

5 5 5 4 4

5 4 4 5

■ '1: 958 € 91

- 16 -

example 2

To determine the properties of the novel products, the products obtained from experiments 1 to 11 were examined above. The moisture content _a, that is to say the proportion of dry material in %, the content of invert sugar and the particle size distribution were determined according to a sieve analysis. Furthermore, the % crystallinity of each product was determined by the usual X-ray diffraction method, using a commercially available sample of crystalline sucrose as the standard measure for 100 % crystallinity. The results of these tests are shown in Table II below.

BAO ORi

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Table II

attempt
No. 1 Dry
substance
in $ Invert
sucker
In % 2 99.95 <1 3 99.5 <i 4th 99.3 6.5 => 99.1 10.6 3O 6th 99.1 14.3 O
Tt 7th
8th 99.2 3.3 "*»
-1
* »
Tl 9 99.1
99.2 11 * 5
7-1 10 99.3 16.2 11th 99.1 5.2 98.9 5.7

Sieve analysis inyu

> 1ÖOO> 5ÖO > 150

> 75

Crystallinity in

2.6 1.6 6.2 42.2 40.0 7.8 2.8 13.4 56.8 24.0 2.8 0 0.2 2.0 11.6 34.6 44.0 8.4 5.9 11.8 36.8 35.2 11.0 0.2 1.8 3.6 15.8 37.4 40.0 1.8 4.2 2.2 5.8 24.8 62.2 1.6

85

85

⁶⁰ 55 70 60 60 85 70 60 55

Example 3

To ensure that the invert sugar / Saooharose sugar product according to the invention can be used in production of sweet chocolate, the sugar obtained in Experiments 9 and 10 became more crystalline with usual Sucrose studied in the manufacture of common so-chocolate overseas mass. Three mixtures were produced

Components Content in wt liquid chocolate 39.120 sugar 48.840 Lecithin 0.350 Ethyl vanillin 0.208 SaIs 0.625 Van Bean Base 0.938 Cocoa butter 11,513

In the three experiments, the sugar was ordered from Experiment A cane sugar (Fig. 1), in experiment B sugar from experiment 9 (Fig. 2) and in experiment C sugar from Trial 10 (Fig. 3) used. To make the mix The procedure was as follows!

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Experiment A; Commercially available sucrose was dry-ground and the fine powdery sugar obtained was then processed with the remaining ingredients in a conventional mixer.

Experiment B: The sugar from Experiment 9 would be mixed with the usual ingredients without intermediate grinding "

Experiment C: The sugar from Experiment 10 was mixed with the other ingredients «

The properties of the products obtained were determined on samples A, B and C, specifically with regard to the smallest particle size in the mixture, the viscosity and fat content; these values are given in Table III below.

Table III 123 Fat content in % Prob Fine fraction · viscosity
in / U in cP 124 34.1 A. 10 136 34.1 B. 10 35.8 C. 10

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BAD ORiGhMAL

~ 20 -

In order to investigate the suitability of these mixtures as a coating mass for chocolate sweets, caramel cores were coated with these masses in the usual way and the quality was determined according to known methods. For the Besehichten been lüoramelliförne- first 1.5 eh "fcungsraasee aufgesoßraol SEN and cooled fees on 2J ° C, ÄnsehlieSißd imjrd © again rwärmt the mass ^ 2 ⁰ C and stirred for 30 seconds © g of broom!. The Kareraellkerae were immersed in the coating composition and anschlieBend cooled at 12 ^Q C in a Künltunnel. The coatings showed a uniform and good consistency, the aging properties of these chocolate candies all in one

investigated, di @ three times in a row for 16 hours at 20 ⁰ G and % iger ϊμ £ tf euchte «iid 8 hours feel 30% and 5§ ^ ig @ r rel & iivur lAiftfeuchte © was set« MSiSh this aging test sausage © found that the usual measures B and Ό with the non-ground sugar S ^ siss ^ f iiidimg di # gl # i5li @% ialifeHt and there «the same« ice cream iseigteas like 1!

With de © erffiii, ci-angsgemässen Verfahrsii are additionally lent «Let Hauen Iri ^ Äifces aifc read and

since practically 4 % of the total sugar content of the starting product is contained in edible solid worm *

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Seconds hsrafo lowered; and no longer amounts to hours, whereby a cararaellization is completely excluded and no longer large ¥ erdarapfungsanlsgen and crystallization pans and means for Eäpzeugimg a vacuum are required.

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Claims (1)

Claims a) in @ in © a HeieLuftetroa ^ etrennfe i ^ igsftlhrt® Saeelsarose- l & mmg wiü fein © fc) the ¥ a @@@? vm the on 0} the coated tailoh ^ i isolated from aeia air flow. Process according to I ₉ dadureh k ^ iBKsIolinöt * that the desi process added sugar particles is a product that has to be rfalsren after Anepruuh I to S ,. daat ^ öh marked, that the SßöehÄros®li5simg from a decolorized and desalinated Rohrauskerrohslrup confirmed. 4 «Method according to claim I to S, characterized in that it is identified, that the Sacoharos © 18aung consists of a decolorized and desalted Saaeharoee syrup, which contains noticeable proportions of invert sugar » 5 · Procedure! nmh claim 1 to 4, thereby s & et, d && sian carries out the process in a spray drying of the zeolite type. According to claims 1 to 5, it is characterized by the fact that the solid material supplied is in a range of 1 to 4 times the weight of the solid components of the liquid input product. 7 · Ycirfaiaren Nmth claims 1 to 5, characterized in that * the weight entspriclit NiAl weight of the solids in the liquid to solid Einsatzxeaterlal feedstock 2 to 3 » 8 »The method of claim 1 to 7 characterized in _{# B} üte Äustrlttstemperatur in the range of 55 to 75 ° C 009825/1353